GdBO3:Ln(3+) (Ln = Eu, Tb) nanofibers were synthesized using electrospinning combined with heat treatment. The synthesized nanofibers were characterized by X-ray diffraction, Raman spectroscopy, field emission-scanning electron microscopy, thermogravimetric and differential thermal analyses, and photoluminescence. The experimental results show that the flexible synthesized nanofibers have an average diameter of approximately 150 nm. The nanofibers consist of crystalline grains with diameters of about 40 nm and have a vaterite-type structure of GdBO3. The GdBO3:Eu3+ nanofibers exhibit strong orange and weak red emissions with a low ratio of red to orange emission intensities, which is different from those of the reported bulk materials and nanoparticles. The luminescence properties of the synthesized GdBO3:Tb3+ nanofibers are essentially consistent with those of the synthesized GdBO3:Tb3+ powders by solid-state reaction. (C) 2012 Elsevier B.V. All rights reserved.